Vanadium compound and method of making same



Patented 6, 19 27.

1 UNITED STATES; PATENT orno-E. i

. mnnr c. snap, on mew YORK, 1w. 1., nssrcmon or ons-rump ro rao u s corrnn, or masnrcrrr, mew JERSEY, nun oNn-rnran 'ro smear L. mama, or 'cnnnn- I vlmamun comrounn m unrnon or inaxmesamn.

I !o Drawing 5 This intention relates to the art of. re-

covery of'metals, and particularly has ref-' erence'to the recovery of vanadium fro'ma groduct of combustion, resulting'f'iromthe roduct 'resultin urningof petro eum. I have discovered that the residue, or

from .the combustion or urnin of etroleum, cont'ains- 'vanadium,

.- the sai resi us, or product, bein commonly g. =known as'soot or-flue dust whic collects in :thestacks or chimneys of buildings, shi s,

.,;; furnaces and in the retor'ts-andonthe e.

sides. of the boilers and tubes of oil burning a paratus andinstallations. The burns in ogpetroleum also produces a substance, w -'ch is neither soot nor flue-dust, as a deposit. injthe retorts, on the boilers," tubes,"

deposit resulting from the combustion of .30 petroleum, regardless of the apparatus in which. the oil is burned, I have discovered,

also, that the .said deposit contains radium and; uranium; but,since, according .to my discovery, vanadiumis found in higher percentage," my invention. primarily. relates to the recovery of vanadium, and the rocess with which I have experimented" is irected. more particularly to the recovery of vana dium than of the other metals; a 40 In order to demonstrate my discovery, I have subjected large uantities of petroleum soot to' treatment an have been successfulin obtaining vanadium compounds therefrom, .toge ther with; alloys thereof. There .45 fore, myinyention consists in the method I or process of. .recoverinvanad11}m from t eptoduct of said petroleum" soot,, and in process, both; immediate and mediate, as hereinafterfdescribed andclaim'ed.

I trinfiform the bulk. soot recoverymtyanadium is as follows":

the presence of heat.

forms of deposits,

other metals of the hydrogen sulphide grou 1 The P DGBSS I have employed in the carnotite, said further steps being substanto bri-" e to conveniently and prop-- appl cation filed February 20, 1924. s m No. canoes.

erly handled. Or, first, I roast the soot in a rotar kiln; but, I conceive that the roasting may e carried out b other means v .or apparatus. This roasting e inates most of the sulphur and carbon and markedly reduces the material both in bulk and wei ht;

To transform thebulk, eitherroaste or unroasted, into briquettes, I mix the bulk with a binder in su table proportions, such as sodium silicate solution, and subject the mixture'to ressure, or its equivalent,,in a 5 sultable mo d' or chamber, with 01 without In this connection, I place no limit upon the size of the briq uette, or cake,'or block, formed, since the limitations imposed, inany event, will have reference to convenience and facility in handling. When the briquette is formed or made'if the bulk has not been roasted, the

-briquette may be roasted. I wish it' understood, however, that it is notan-essential of my process that the bulk or briquette should .be roasted; nor is it an essential of my process that the bulk material should be transformed into briquettes, blocks, or cakes.

The roasted or unroastedmaterial or briquette is then fused to bring the vanadium into solution; or it may be leached at desired-temperature with either acid or alkaline solution. As an example of a means for this purpose I may use a fusion with approximate y three or four times its weight of nter cake. The fused mass, after-cooling, is broken up and leached with water. The solution thus produced is filtered irom the insoluble residue. The filtered solution will contain a large percentage of the vanadium present in the soot. L

The solution is treated with hydrogen sulphide to remove molybdenum, copperand which may be present. T e precipitatedsu phides are removed by filtration and the, clear solution is heated, air being blown in to remove the H S. 4

The solution thus obtained is then treated generally according to the process pre-' scribedby the Bureau of Mines in its Bulletin 104, Mineral Technology 12-, for'the extraction and recovery of vanadium from tially as follows: F

The solution, containing the vanadium and any uranium present, is run slowly with sodium carbonate.

solution is strongly alkaline.

' roasted soot treated. The solution is boiled for from two to three hours after the final addition of the blue acid solution to completely precipitate the iron, cromium, aluminum, etc., and is then filtered. If the amount of excess carbonate and the time of boiling are carefully checked and controlled the precipitate will be reasonably free from vanadium. The filtrate from the iron precipitate is neutralized with HNO, the solution being left just neutral. Air is blown through the boiling solution to remove CO .A solution of ferrous sulphate is added to recipitate the vanadium as iron vanadate. gince the addition of the sulphate will leave the solution slightly acid, enough NaOH is added to again make it neutral. The precipitate will be yellow, brown or graygreen according to the conditions under which the precipitation was made and will contain from 25 to per cent of V 0 The solution is filtered and the iron vanadate precipitate washed and dried. The precipitate may be reduced to 'ferrovanadium or may be treated by other suitable means to secure other vanadium compounds or alloys, which are in a form for commercial use.

By variations or modifications of the foregoing process, I may also obtain oxide of vanadium or vanadate precipitate, and other compounds and alloys of vanadium, as an article of manufacture or commercial prod,-

not, my particular product resulting from the foregoing process being, as just stated,

ferrovanadium.

Lmay also produce a concentrate containing vanadium by, suspending the soot in water, or producing a water and soot mixture, to render it limpid and capable of bein readily poured or of flowing. The limpid mixture is then putthrough a classifier, the overflow carrying oil the soot and lighter materials; that is to say, the specific gravity of the diiferent constituents is utilized to separate the same. I thenrun the precipitate over a concentrator. The product is a concentrate containing vanadium.

In the foregoing i haveset forth the process employed by me in the recovery of vanadium from petroleum soot, and desire to lay stress thereon and upon the products thereof in addition to my primary discovery of vanadium in the soot of petroleum resulting from combustion thereof. .1 also desire to- 1ay stress u n my primary product, .viz, briquette, or look, vanadium-containing soot which 'ves immediate commerciality to my discovery, since it enables binder.

me to convey the vanadium-containing soot directly to the users of large quantities of soot for the production of commercial vanadium, and in this connection I desire it understood that I realize that more satisfactory commercial results may be obtained in a commercialized plant, such as v a direct smelter, than I have obtained as the result of the limitations imposed upon me in ogrrying out and developing my invention resulting from my primary and very important discovery.

Having thus described my invention, what I claim and desire to secure by Letters Pat out is:

of the products of combustion of petroleum characterized by its content of vanadium.

2. As an article of manufacture, a. residue of the products. of combustion of etroleum characterized by its content of errovanadium.

3. As an article vof manufacture, a residue of the products of combustion of petroleum characterized by its content 'of oxide of vanadium. v

l. The method of deriving vanadium precipitate from the products. of combustion of petroleum, including treating said products by concentration.

1. As an article of manufacture, a residue 5. As a new article of manufacture a briquette composed of the soot resulting from the burning or combustion of petroleum.

6. The method of recoverin vanadiumbearing substances-from the products of combustion of petroleum by means of mechanical concentration.

7. The method of deriving vanadium preoipitate from petroleum, comprising the production of soot from the petroleum and chemically treating the soot to produce a precipitate.

8. The method of recovering vanadiuin' or a precipitate thereof from petroleum, comprising producing soot from petroleum by burning the latter; and fusing and leaching the soot to produce ferrovanadium, oxide of vanadium, a vanadate precipitate, and other compounds.

9. The method herein described of recov ermg vanadium from petroleum soot, comprising roasting the soot; fusingv the roasted material with nitercake; leaching the fused mass; and filtering the solution.

10. The method herein described of producing a vanadium compound from petroleum soot, comprising producing a hmpid mixture of soot and water; subjectin the lim'pid mixture to the action of a classlfier; and subjecting the precipitate to the action 11. As a new article of manufacture a briquette composed of petroleum soot and a 12. The

method of making a briquette of 1,e 1,ee7 r r B soot of ,petroleum comprising mixing the 14. A process for recovering v anadium soot with a binder, and subjecting the mixfrom petroleum hydrocarbons, consisting in ture to pressure to give it a definite form. exhausting hydrocarbon products by com- 13. The method of making a briquette of bustion and collecting the deposited vanadi- 5 soot of petroleum comprising mixing the um compounds.

soot with a binder, and molding the mixture into predetermined form ALBERT 

